CN101898791A - Method for preparing rutile titanium dioxide from new process titanium slag - Google Patents
Method for preparing rutile titanium dioxide from new process titanium slag Download PDFInfo
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Abstract
The invention discloses a method for preparing titanium dioxide from new process titanium slag, and belongs to the technical field of titanium dioxide production. The method comprises the following steps of: performing acidolysis reaction on the new process titanium slag and concentrated sulfuric acid under certain conditions; leaching, precipitating and filtering the mixture to obtain clear titanium liquid; adding an aluminum removing agent into the clear titanium liquid to recover aluminum by freezing crystallization; adding oxidized trivalent titanium serving as an oxidant into the clear titanium liquid and concentrating the mixture; hydrolyzing, filtering and washing the concentrate by using a process for adding crystal seeds; and bleaching, salting, calcining and post-processing the filter cake to prepare the rutile titanium dioxide which meets the application requirement. The method has the most noticeable characteristic that the rutile titanium dioxide which meets the application requirement is prepared from the new process titanium slag which has the disadvantages of various impurities and difficult acidolysis; and thus a new raw material for producing the titanium dioxide by a sulfuric acid method is developed, various valuable elements are recovered as much as possible, the utilization ratio of the resource is improved and the production cost is reduced.
Description
Technical field
The present invention relates to a kind of preparation method of titanium dioxide, specifically, relate to a kind of method of utilizing the new technological process titanium slag to prepare the rutile titanium white powder, belong to the titanium white production technical field.
Background technology
Titanium dioxide formal name used at school titanium dioxide (TiO
2), be a kind of important white pigment and porcelain glaze, be widely used in aspects such as metallurgy, coating, plastics, papermaking, printing ink, synthon, rubber, welding electrode, electrical condenser, electroceramics, makeup, opaquing fluid.The commodity of titanium dioxide have two kinds of rutile-type (Rutile R type) and anatase titanium dioxides (Anatase A type), the densification of rutile-type crystalline structure, and relative density is bigger, and is more stable, and optical activity is little, thereby good weatherability, higher opacifying power is arranged simultaneously, reducing power; The anatase titanium dioxide relative density is less, and photostabilization is relatively poor.
The production method of titanium dioxide mainly contains two kinds of sulfuric acid process and chlorination processs.Wherein sulfuric acid process can be used for producing anatase titanium dioxide and Rutile type Titanium Dioxide.Owing to reasons such as raw material sources and technology, the China's titanium white powder enterprise overwhelming majority adopts sulfuric acid process.
The main flow process of the technology of sulfuric acid method titanium pigment production comprises, ilmenite concentrate or acid-dissolved titanium slag and the vitriol oil are carried out acidolysis reaction generate titanium sulfate and titanyl sulfate, acid hydrolysis solution is removed the ferrous titanium liquid clearly that obtains through settlement separate solid impurity, freezing and crystallizing, after concentrating, clear titanium liquid generates hydrated titanium dioxide (metatitanic acid) through hydrolysis again, metatitanic acid by technologies such as calcining, middle pulverizing and aftertreatments, obtains the titanium dioxide product after rinsing, salt are handled.The main raw material of sulfuric acid process is ilmenite concentrate and acid-dissolved titanium slag.Ilmenite concentrate is many to get its TiO by natural various ilmenites through multiple flotation
2Content is generally 47%-55%, and grade is lower.To be ilmenite remove the rich titanium material that a kind of available sulfuric acid that most of iron forms decomposes, its TiO through electrosmelting (reducing roasting) to acid-dissolved titanium slag
2Content is 75%-85%, and is of high grade, and foreign matter content is few, is the development trend of current international titanium material.
Except ilmenite, the v-ti magnetite ore resources is rich in China, and only the identified vanadium titano-magnetite ore reserves of Panxi Diqu has reached 10,100,000,000 tons.For the comprehensive utilization of vanadium titano-magnetite, traditional method mainly adopts " blast furnace-converter " flow process to smelt, and make iron and vanadium in the complex ore obtain utilizing preferably, yet wherein the titanium resource more than 50% has directly entered blast furnace slag, is difficult to be utilized.For the ferrovanadium titanium in the comprehensive reutilization complex ore better, Chinese patent CN101619371 discloses a kind of method that reclaims the vanadium ferrotianium from vanadium titano-magnetite, with the vanadium titano-magnetite breeze with coal dust, caking agent agglomeration, reduction obtains metallized product under 1300-1400 ℃ temperature in rotary hearth furnace, hot charging enters the furnace melting separation then, obtains vanadium-bearing hot metal and titanium slag.This flow process adopts the molten division technique of rotary hearth furnace coal-based direct reduction-electric furnace, and different with traditional blast furnace-converter technology, the molten minute slag that this technical process obtains mainly is titanium slag, is called the new technological process titanium slag.TiO in the new technological process titanium slag
2Content is more than 50%, and iron oxide content is 2-6%, and pentoxide content is 0.2-0.8%.The main component of new technological process titanium slag and ilmenite concentrate, acid-dissolved titanium slag relatively sees Table 1:
Table 1 new technological process titanium slag, ilmenite concentrate and acid-dissolved titanium slag main component are relatively
| Main component quality percentage composition (%) | Ilmenite concentrate | The new technological process titanium slag | Acid-dissolved titanium slag |
| TFe? | 28-33? | 2-6? | 2-5? |
| TiO 2 | 46-48? | 47-58? | 75-90? |
| V 2O 5 | 0.02-0.2? | 0.2-0.8? | 0.02-0.2? |
| Cr 2O 3 | 0.010-0.1? | 0.1-0.4? | 0.01-0.1? |
| Al 2O 3 | 1-3? | 8-18? | 1-3? |
| SiO 2 | 2-5? | 6-15? | 2-4? |
| CaO? | 0.5-2? | 4.33-10? | 0.2-1? |
| MgO? | 1-3? | 7-12? | 0.5-2? |
As can be seen from Table 1, the grade of titanium is high slightly than ilmenite concentrate in the new technological process titanium slag, but well below acid-dissolved titanium slag; The content of iron is significantly less than ilmenite concentrate, approach acid-dissolved titanium slag, the content of impurity element vanadium, chromium, aluminium, magnesium is more than several times even tens times of ilmenite concentrate and acid-dissolved titanium slag, impurity element chromium, vanadium are the main harmful elements that influences the titanium dioxide quality, and the too high levels of aluminium, magnesium, when clear titanium liquid temp reduced, magnalium and water were combined into crystal (Mg SO
47H
2O, Al
2(SO
4)
318H
2O), it is gelatin to cause dense titanium liquid to be condensed into, and makes to produce to be difficult to carry out continuously, and the content of iron is low, and the content of iron is fewer, and iron reaction liberated heat is just few, therefore initially also needs to provide the part heat that reaction can be kept down at acidolysis reaction.This shows that the new technological process titanium slag is not a kind of desirable feedstock of producing titanium dioxide.
Because the new technological process titanium slag is to separate the molten minute slag that obtains through high temperature melting, through X-ray diffraction analysis, the crystal formation of finding this titanium slag is a kind of chemicals of titanium magnalium mixing crystal formation, complex structure, so will utilize this titanium slag to want that at first the impurity of removing wherein from the source re-uses, can through use dilute sulphuric acid, dilute hydrochloric acid etc. 70-80 ℃ repeatedly dip also be difficult to the minimizing of the content of impurity element vanadium, chromium, aluminium, magnesium is illustrated that this titanium slag is difficult to acidolysis than general acid-dissolved titanium slag.And be the feedstock production titanium dioxide with the new technological process titanium slag directly, adopt common titanium dioxide technology to produce, then being difficult to acidolysis owing to crystalline structure is special finishes, acidolysis rate is low, the titanium liquid of acidolysis gained is then because foreign matter content height wherein, often produce jelly and make production process be difficult to carry out continuously, and the titanium dioxide quality of producing is restricted, only can be as low-quality titanium dioxide, made the coating anatase thpe white powder in the laboratory as Beijing total institute of coloured research in 1989, and the industrial non-pigment titanium white that only can obtain as welding electrode.So far do not find to adopt the new technological process titanium slag to prepare the report of the higher Rutile type Titanium Dioxide of quality.
Summary of the invention
The objective of the invention is to overcome the deficiency that existing new technological process titanium slag in the prior art is difficult to be applied to the high-quality rutile titanium white powder of industrial production, a kind of method of utilizing the new technological process titanium slag for raw material production rutile titanium white powder is provided.Utilize method of the present invention, can produce the qualified rutile titanium white powder of pigment performance.
The present invention realizes that the technical scheme of above-mentioned purpose is as follows:
A kind of method of utilizing the new technological process titanium slag to prepare the rutile titanium white powder comprises the steps:
(1), the acidolysis of new technological process titanium slag:
The new technological process titanium slag is pulverized, and is that 1.65-1.8 adds the vitriol oil by sour ore deposit mass ratio, stirs, and adds ANTIMONY TRIOXIDE SB 203 99.8 PCT (Sb according to the ratio of 1-20kg/ ton new technological process titanium slag
2O
3), mix, adding entry conditioned reaction acid concentration is 93-96%, stop heating after under agitation being warming up to 130-150 ℃, make spontaneous the carrying out of reaction, generate solid mixt, solid mixt is placed 160-220 ℃ of following slaking 3-5h, by water ore deposit mass ratio is 2.5-3: 1 adds the water extraction solid mixt, and leaching temperature is 60-75 ℃, and leaching time is 1-3h;
(2), sedimentation removal of impurities:
Ratio in 10-40kg/ ton new technological process titanium slag in step (1) gained acid hydrolysis solution adds FeS, and the ANTIMONY TRIOXIDE SB 203 99.8 PCT that adds when FeS and acidolysis forms sinking agent, and sedimentation goes out most chromium metal, vanadium in the acid hydrolysis solution; Add flocculation agent again, make short grained solid impurity sedimentation, after solid-liquid separation, obtain titanium liquid clearly, in clear titanium liquid, add aluminum removal, freezing and crystallizing 1-2h under 10-20 ℃ temperature, add aluminum removal molar weight be Tai-Ace S 150 mole number in the solution 1.0-1.5 doubly;
The separation of freezing and crystallizing after-filtration obtains crystal and titanium concentration is the titanium liquid of 110-140g/L, adds oxygenant in described titanium liquid, makes the concentration of the titanous in the titanium liquid reduce to 1-2g/L by 5-20g/L; Gained liquid obtains the dense titanium liquid that concentration is 200-235g/L through concentrating after the oxidation;
(3), hydrolysis:
In the dense titanium liquid of step (2) gained, add automatic growing crystal species or plus seed and be hydrolyzed, add plus seed quality be TiO in the titanium liquid
2The 1-3% of quality; Titanium liquid initial reaction concentration is 180-195g/L, and the temperature that adds crystal seed is 90-95 ℃;
(4), filter, wash:
With the hydrolysis slurry filtration of step (3) gained, the filter cake that obtains obtains the rutile titanium white powder after bleaching, salt processing, calcining, aftertreatment.
Above-mentionedly utilize in the method that the new technological process titanium slag prepares the rutile titanium white powder the preferred 1.67-1.75 of sour ore deposit mass ratio in the step (1), the preferred 95%-96% of reaction acid concentration, preferred 3-4h of curing time.
The above-mentioned utilization in the method that the new technological process titanium slag prepares the rutile titanium white powder, described new technological process titanium slag preferred powder are broken to proportion of particles greater than 45 microns (325 mesh sieves) less than 15%.
The above-mentioned utilization in the method that the new technological process titanium slag prepares the rutile titanium white powder, flocculation agent described in the step (2) are the poly-propionic acid amide of the general formaldehyde dimethylammonium modification of titanium dioxide producer.
The consumption of the poly-propionic acid amide of the described formaldehyde dimethylammonium of step (2) modification is 15-30ppm.
Aluminum removal is ammonium sulfate or vitriolate of tartar described in the step (2), and it is Tai-Ace S 150 or potassium aluminium sulfate crystal that the freezing and crystallizing after-filtration separates the crystal that obtains.This crystal is as the byproduct of present method.
Oxygenant is oxygenants such as Sodium Nitrite or SODIUMNITRATE described in the step (2).
The above-mentioned utilization in the method that the new technological process titanium slag prepares the rutile titanium white powder, the quality that adds crystal seed in the step (3) is TiO in the titanium liquid
2The 1.5-2.5% of quality.
Institute adds crystal seed preferentially to adopt plus seed is the titanium tetrachloride crystal seed in the step (3).
Because the new technological process titanium slag is to separate the molten minute slag that obtains through high temperature melting, wherein contain impurity such as higher chromium, vanadium, aluminium, magnesium, silicon, calcium and make acidolysis reaction condition harshness, the easy crystallization of the titanium liquid that produces produces colloid makes production be difficult to carry out continuously the titanium white powder pigment poor-performing of production.The inventor is through repetition test, optimize the reaction conditions of acidolysis, for the new technological process titanium slag of solubility in acid difference, the condition of constantly groping acidolysis reaction not only will make reaction take place, continue to carry out and complete reaction, obtain the acidolysis rate of higher titanium, and as far as possible the acidolysis of impurity selectivity, invalid silicon, calcium etc. are not reacted substantially, few as far as possible reaction such as chromium, vanadium, aluminium, must select suitable sour ore deposit ratio, suitable reaction acid concentration.After the acidolysis main reaction, in order to strengthen effect of settling, the contriver has added Sb
2O
3And FeS, make acidolysis, sedimentation integrated, Sb
2O
3The SbS that generates with FeS has reasonable effect to the sedimentation of heavy metal elements such as chromium, vanadium, and the poly-propionic acid amide of flocculation agent formaldehyde dimethylammonium modification is obvious to micromolecular suspended substance effect, these two kinds of sedimentation methods are used in combination, both can be the suspended substance sedimentation of trying one's best, again can as far as possible will be to the severe heavy metal element sedimentation of pigment influence.
Because still contain higher aluminium, magnesium in the clear titanium liquid that sedimentation end filtering separation obtains, when temperature reduced, magnalium can be combined into crystal (Mg SO with water
47H
2O, Al
2(SO
4)
318H
2O), cause dense titanium liquid to be condensed into paste, make to produce to be difficult to carry out continuously.The contriver finds that after deliberation after the adding aluminum removal was removed aluminium, the magnesium of Individual existence was difficult to be combined into crystal with water and hinders production, so contriver's adding aluminum removal in clear titanium liquid is removed aluminium and kept the magnesium favourable to product.Through repetition test, the contriver finds that the Tai-Ace S 150 in the titanium liquid can react production exsiccated ammonium alum or potassium aluminium sulfate with ammonium sulfate or vitriolate of tartar, and simultaneously owing to exist the chromium element in the titanium liquid, be easy to generate ammonium chromic sulfate, can cause like this containing this deleterious element of chromic salts in the crystal of the by product exsiccated ammonium alum that obtains or potassium aluminium sulfate and influenced application performance.Through threshing simultaneous test, the contriver finds that exsiccated ammonium alum or potassium aluminium sulfate crystalline solubleness reduce relatively more severely along with the reduction of temperature, ammonium chromic sulfate then changes not quite, so the experimental selection of contriver by repeatedly suitable temperature, concentration conditions, obtain ammonium sulfate or vitriolate of tartar as aluminum removal, removed the method for most of aluminium by freezing and crystallizing.
The present invention can adopt automatic growing crystal species or the plus seed hydrolysis can, the preferential plus seed method for hydrolysis of selecting, and crystal seed is selected the titanium tetrachloride plus seed, and (preparation of titanium tetrachloride crystal seed and plus seed method for hydrolysis are seen, Tang Zhenning, titanium white production and environmental improvement, the P119-126 page or leaf), because this crystal seed preparation does not need impure many titanium liquid, but adopt the titanium tetrachloride aqueous solution preparation, can obtain purified crystal seed, selection by proper hydrolyzing condition, pH condition during hydrolysis particularly, the selection of hydrolyzate concentration can suppress chromium as far as possible, the hydrolysis of vanadium, the metatitanic acid that obtains when making hydrolysis is impure few, the hydrolysis slip that obtains is easier of the impurity washes clean, and the product pigment performance of gained is relatively good.With respect to plus seed, the crystal seed of automatic growing crystal species is to generate at the beginning of the titanium hydrolysis, because titanium liquid own is impure many, the crystal seed of production is impure, and the hydrolysis slip that obtains is impure many, is difficult to washes clean.So the present invention preferentially adopts titanium tetrachloride plus seed method.
Compared with prior art, beneficial effect of the present invention:
(1) many impurity, acidolysis is difficult, the new technological process titanium slag that is not suitable for producing titanium white is applied in the production of titanium dioxide after removal of impurities is reclaimed, and has prepared the rutile titanium white powder that reaches application requiring;
(2) developed a kind of new raw material of titanium white production, the titanium slag not high to some titanium grades, being difficult to provides the application thinking with the raw material that usual method is used;
(3) accomplished comprehensive utilization, reclaimed various valuable elements as far as possible, improved the utilization ratio of resource, thereby reduced production cost.
Description of drawings: Fig. 1 is a process flow diagram of the present invention.
Embodiment
The present invention is described in further detail below in conjunction with testing example and embodiment.But this should be interpreted as that the scope of the above-mentioned theme of the present invention only limits to following embodiment, allly all belong to scope of the present invention based on the technology that content of the present invention realized.
The main component of ilmenite concentrate described in Comparative Examples that the present invention enumerates and the embodiment and new technological process titanium slag sees Table 2.
Table 2 Comparative Examples, embodiment raw material main component
| Project | TiO2? | TFe? | CaO? | MgO? | Al2O3? | SiO2? | Cr 2O 3 | V 2O 5 |
| Comparative Examples 1 | 47.56? | 28.74? | 1.15? | 2.78? | 1.89? | 3.96? | 0.01 2? | 0.058? |
| Comparative Examples 2 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 1 | 47.08? | 4.81? | 13.80? | 12.94? | 15.58? | 12.18? | 0.12? | 0.36? |
| Embodiment 2 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.28? | 0.56? |
| Embodiment 3 | 56.35? | 2.95? | 3.21? | 9.47? | 9.78? | 8.56? | 0.40? | 0.87? |
| Embodiment 4 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 5 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 6 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
Comparative Examples 1
The vitriol oil of 1683 grams 98% is put into the beaker of 5000mL by sour ore deposit mass ratio 1.65, add while stirring 1000g be crushed to granularity greater than 45 micron particle ratios less than 15% ilmenite concentrate (main component of ilmenite concentrate sees Table 2), after mixing, adding 281g water conditioned reaction acid concentration is 84%; Heat temperature raising while stirring then, when temperature rises to 150 ℃, stop heating, reaction will spontaneously be carried out, and generate solid-phase mixture at last, be placed under 180 ℃ the condition slaking 1.5 hours, add water 2500mL leaching, keep 70 ℃ of the temperature of leaching, leaching time is 4 hours, adds the 30g iron powder behind the leaching 2.5h and reduces.
After finishing, leaching adds poly-propionic acid amide (the n formaldehyde: n dimethylamine: polyacrylamide=0.9: 1: 1 of 15ppm flocculation agent dimethylammonium modification, the hydroxymethylation time is 3h, temperature of reaction is 30 ℃) carry out sedimentation, filtering separation obtains titanium liquid clearly, again clear titanium liquid is refrigerated to 16 ℃, crystallization 1 hour, remove ferrous after, concentrate and to make 2 liters of the dense titanium liquid that concentration is 230g/L.
Adding the plus seed titanium tetrachloride in gained titanium liquid is hydrolyzed, add the titanium tetrachloride crystal seed quality be in the dense titanium liquid titanium dioxide quality 2%, hydrolysis temperature is 90-95 ℃, titanium liquid initial reaction concentration is 190g/L, with 60-70 ℃ hot water the metatitanic acid that hydrolysis obtains is washed, the filter cake after the washing is under 65 ℃, and the vitriol oil and the 1.5g/L titanous that add 70g/L are bleached, adopt 60 ℃ hot water that impurity is washed away then, add P more respectively
2O
5/ TiO
2Ratio is 0.2 phosphoric acid, K
2O/TiO
2Ratio is 0.28 potassium hydroxide, Al
2O
3/ TiO
2Ratio is that 0.26 Tai-Ace S 150 carries out salt and handles, and sends to after salt is handled under retort furnace at 980 ℃ of calcining 2h, carries out surface treatment again after grinding, and prepares superior in quality pigment-grade rutile type titanium dioxide finished product 440g, and pigment performance sees attached list 3.
Comparative Examples 2
With the new technological process titanium slag be crushed to granularity greater than 45 micron particle ratios less than 15%, get new technological process titanium slag powder 1000g (composition sees Table 2), than 1.75 1785 grams, 98% the vitriol oil is put into the beaker of 5000mL by sour ore deposit, add the titanium slag powder then while stirring, after mixing, adding 77g water conditioned reaction acid concentration is 96%; Heat temperature raising while stirring when the temperature liter causes 150 ℃, stops heating then, reaction will spontaneously be carried out, and generate solid-phase mixture at last, be placed under 200 ℃ the condition slaking 3 hours, add water 2500mL leaching, keep 70 ℃ of the temperature of leaching, leaching time is 2 hours.
Leaching is finished the poly-propionic acid amide (with Comparative Examples 1) of adding flocculation agent formaldehyde dimethylammonium modification and is carried out sedimentation, filtering separation obtains titanium liquid clearly, after adding the 190g vitriolate of tartar titanium liquid was cooled to 15 ℃ of freezing and crystallizings 1 hour, filtering separation obtains qualified byproduct potassium aluminium sulfate of about 500g and titanium liquid; In gained titanium liquid, add the 150g Sodium Nitrite titanous in the titanium liquid is oxidized to 2g/L, concentrate titanium liquid and make 2 liters of the dense titanium liquid that concentration is 200g/L.
Adopt titanium tetrachloride plus seed technology that gained titanium liquid is hydrolyzed, filter cake after the washing is bleached, washing and salt are handled, calcining, again through aftertreatment (this segment process flow process is with Comparative Examples 1), prepare the rutile titanium white powder finished product 490g that quality reaches application requiring, the yield of titanium dioxide is 87% (pigment performance sees attached list 3) in the new technological process titanium slag.
Embodiment 1
Get be crushed to granularity greater than 45 micron particle ratios less than 15% new technological process titanium slag 1000g (composition sees Table 2), the vitriol oil of 1683 grams 98% is put into the beaker of 5000mL by sour ore deposit mass ratio 1.65, add the titanium slag powder then while stirring, after then adding 1 gram Sb2O mixing, adding 35g water conditioned reaction acid concentration is 96%; Heat temperature raising while stirring when the temperature liter causes 150 ℃, stops heating then, reaction will spontaneously be carried out, and generate solid mixed phase thing at last, be placed under 200 ℃ the condition slaking 4 hours, add water 2500mL leaching, keep 70 ℃ of the temperature of leaching, leaching time is 2 hours.
After finishing, leaching adds 2 gram FeS earlier, add the poly-propionic acid amide (with Comparative Examples 1) of 15ppm flocculation agent formaldehyde dimethylammonium modification again and carry out sedimentation, filtering separation obtains titanium liquid clearly, after adding 150g ammonium sulfate solution is cooled to 12 ℃ of crystallizations 1 hour, filtering separation obtains about 450g exsiccated ammonium alum and titanium liquid, reclaims the gained exsiccated ammonium alum; In gained titanium liquid, add the 150g Sodium Nitrite titanous is oxidized to 2g/L, concentrate and make 2 liters of the dense titanium liquid that concentration is 200g/L.
Adding the plus seed titanium tetrachloride in the dense titanium liquid of gained is hydrolyzed, add titanium tetrachloride quality be in the dense titanium liquid titanium dioxide quality 2%, hydrolysis temperature is 90-95 ℃, titanium liquid initial reaction concentration is 190 g/L, with 60-70 ℃ hot water the metatitanic acid that hydrolysis obtains is washed, filter cake after the washing is bleached, washing and salt are handled, calcining, again through aftertreatment (this segment process flow process is with Comparative Examples 1), obtain rutile titanium white powder finished product 430g, the yield of titanium dioxide is 86% in the new technological process titanium slag, and pigment performance sees attached list 3.
Find by subordinate list, to embodiment 1, at chromium, vanadium, aluminium when not being very high, to product the pigment performance influence little, the pigment performance of gained is near Comparative Examples 1.
Embodiment 2
Get new technological process titanium slag powder 1000g (composition sees Table 2), other prepares the rutile titanium white powder finished product 490g that quality reaches the various performances of application requiring with embodiment 1, and the yield of titanium dioxide is 86% in the new technological process titanium slag, and pigment performance sees attached list 3.
By table 3 as seen, to present embodiment, chromium, vanadium, aluminium content are than embodiment 1 height, and bigger to the pigment performance influence of product, the pigment performance of gained is poorer slightly than embodiment 1.
Embodiment 3
Get new technological process titanium slag powder 1000g (composition sees Table 2), other prepares the rutile titanium white powder finished product 510g that quality reaches the various performances of application requiring with embodiment 1, and the yield of titanium dioxide is 86% in the new technological process titanium slag, and pigment performance sees attached list 3.
Found that by table 3 to present embodiment, chromium, vanadium, aluminium content are than embodiment 2 height, bigger to the pigment performance influence of product, the pigment performance of gained is poorer than embodiment 2, admittedly require the content of chromium, vanadium, aluminium impurity of new technological process titanium slag low as far as possible.
Embodiment 4
Get be crushed to granularity greater than the ratio of 45 microns (325 mesh sieves) less than 15% new technological process titanium slag 1000g (composition sees Table 2), than 1.75 1785 grams, 98% the vitriol oil is put into the beaker of 5000mL by sour ore deposit, add the titanium slag powder then while stirring, after then adding 1 gram Sb2O mixing, then adding 38g water conditioned reaction acid concentration is 96%; Heating while stirring then when the temperature liter causes 150 ℃, stops heating, reaction will spontaneously be carried out, and generate solid-phase mixture at last, be placed under 210 ℃ the condition slaking 4 hours, add water 2500mL leaching, keep 75 ℃ of the temperature of leaching, leaching time is 1.5 hours.
After finishing, leaching adds 2 gram FeS earlier, add the poly-propionic acid amide (with Comparative Examples 1) of 15ppm flocculation agent formaldehyde dimethylammonium modification again and carry out sedimentation, filtering separation obtains titanium liquid clearly, after adding 150g ammonium sulfate solution was cooled to 12 ℃ of freezing and crystallizings 1 hour, filtering separation obtains qualified exsiccated ammonium alum byproduct of about 450g and titanium liquid; In gained titanium liquid, add the 150g Sodium Nitrite titanous is oxidized to 2g/L.Concentrate and to make 2 liters of the dense titanium liquid that concentration is 200g/L.
Adding the plus seed titanium tetrachloride in the dense titanium liquid of gained is hydrolyzed, add titanium tetrachloride quality be in the dense titanium liquid titanium dioxide quality 2%, hydrolysis temperature is 90-95 ℃, titanium liquid initial reaction concentration is 190g/L, with 60-70 ℃ hot water the metatitanic acid that hydrolysis obtains is washed, filter cake after the washing is bleached, washing and salt are handled, calcining, again through aftertreatment (this segment process flow process is with Comparative Examples 1), prepare the rutile titanium white powder finished product 500g that quality reaches application requiring, the yield of titanium dioxide is 88% in the new technological process titanium slag, and pigment performance sees attached list 3.
Find and embodiment 2 contrasts by subordinate list 3, present embodiment material content unanimity, but changed acidolysis and slaking condition, the pigment performance of gained is better slightly than embodiment 2.
Embodiment 5
Get new technological process titanium slag powder 1000g (composition sees Table 2), than 1.75 1785 grams, 98% the vitriol oil is put into the beaker of 5000mL, add the titanium slag powder then while stirring, then add 1 gram Sb by sour ore deposit
2After O mixed, adding 77g water conditioned reaction acid concentration was 94%; Heat temperature raising while stirring when the temperature liter causes 140 ℃, stops heating then, reaction will spontaneously be carried out, and generate solid-phase mixture at last, be placed under 180 ℃ the condition slaking 3 hours, add water 2500mL leaching, keep 65 ℃ of the temperature of leaching, leaching time is 3 hours.
After finishing, leaching adds 2 gram FeS earlier, add the poly-propionic acid amide (with Comparative Examples 1) of 20ppm flocculation agent formaldehyde dimethylammonium modification again and carry out sedimentation, filtering separation obtains titanium liquid clearly, after adding 150g ammonium sulfate solution is cooled to 12 ℃ of freezing and crystallizing 1h, filtering separation obtains qualified exsiccated ammonium alum byproduct of about 450g and titanium liquid; In gained titanium liquid, add the 150g Sodium Nitrite titanous is oxidized to 2g/L.Concentrate and to make 2 liters of the dense titanium liquid that concentration is 200g/L.
Adding self crystal seed is hydrolyzed in the dense titanium liquid of gained, add crystal seed quality be in the dense titanium liquid titanium dioxide quality 2.5%, hydrolysis temperature is 90-95 ℃, titanium liquid initial reaction concentration is 190g/L, with 60-70 ℃ hot water the metatitanic acid that hydrolysis obtains is washed, filter cake after the washing is bleached, washing and salt are handled, calcining, again through aftertreatment (this segment process flow process is with Comparative Examples 1), prepare the rutile titanium white powder finished product 490g that quality reaches application requiring, the yield of titanium dioxide is 87% in the new technological process titanium slag, and pigment performance sees attached list 3.
Find and embodiment 2 contrasts by subordinate list 3, present embodiment material content unanimity, but changed acidolysis, slaking condition, and having adopted the automatic growing crystal species hydrolysis, the pigment performance of gained is poorer than embodiment 2.
Embodiment 6
Get new technological process titanium slag powder 1000g (composition sees Table 2), than 1.75 1785 grams, 98% the vitriol oil is put into the beaker of 5000mL by sour ore deposit, add the titanium slag powder then while stirring, after then adding 1 gram Sb2O mixing, adding 77g water conditioned reaction acid concentration is 94%; Heat temperature raising while stirring when the temperature liter causes 150 ℃, stops heating then, reaction will spontaneously be carried out, and generate solid-phase mixture at last, be placed under 200 ℃ the condition slaking 3 hours, add water 2500mL leaching, keep 70 ℃ of the temperature of leaching, leaching time is 2 hours.
After finishing, leaching adds 2 gram FeS earlier, add the poly-propionic acid amide 20ppm of flocculation agent formaldehyde dimethylammonium modification again and carry out sedimentation, filtering separation obtains titanium liquid clearly, behind the adding 190g vitriolate of tartar solution is cooled to 15 ℃ of freezing and crystallizings 1 hour, filters and obtains qualified potassium aluminium sulfate byproduct of about 500g and titanium liquid; In gained titanium liquid, add the 150g Sodium Nitrite titanous is oxidized to 2g/L.Concentrate and to make 2 liters of the dense titanium liquid that concentration is 200g/L.
Adding the plus seed titanium tetrachloride in the dense titanium liquid of gained is hydrolyzed, add titanium tetrachloride quality be in the dense titanium liquid titanium dioxide quality 1.5%, hydrolysis temperature is 90-95 ℃, titanium liquid initial reaction concentration is 190g/L, with 60-70 ℃ hot water the metatitanic acid that hydrolysis obtains is washed, filter cake after the washing is bleached, washing and salt are handled, calcining, again through aftertreatment (this segment process flow process is with Comparative Examples 1), prepare the rutile titanium white powder finished product 490g that quality reaches application requiring, the yield of titanium dioxide is 87% in the new technological process titanium slag, and pigment performance sees attached list 3.
Find and embodiment 5 contrasts by subordinate list 3, present embodiment material content unanimity, but change aluminum removal and remove aluminum strip spare, the pigment performance of gained is more similar than embodiment 2.
Table 2 embodiment new technological process titanium slag main component
| Project | TiO2? | TFe? | CaO? | MgO? | Al2O3? | SiO2? | Cr 2O 3 | V 2O 5 |
| Comparative Examples 1 | 47.56? | 28.74? | 1.15? | 2.78? | 1.89? | 3.96? | 0.012? | 0.058? |
| Comparative Examples 2 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 1 | 47.08? | 4.81? | 13.80? | 12.94? | 15.58? | 12.18? | 0.12? | 0.36? |
| Embodiment 2 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.28? | 0.56? |
| Embodiment 3 | 56.35? | 2.95? | 3.21? | 9.47? | 9.78? | 8.56? | 0.40? | 0.87? |
| Embodiment 4 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 5 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
| Embodiment 6 | 53.35? | 3.88? | 3.50? | 10.42? | 8.42? | 10.27? | 0.24? | 0.56? |
The pigment performance of table 3 embodiment titanium dioxide
Claims (8)
1. a method of utilizing the new technological process titanium slag to prepare the rutile titanium white powder is characterized in that comprising the steps:
(1), the acidolysis of new technological process titanium slag:
The new technological process titanium slag is pulverized, and is that 1.65-1.8 adds the vitriol oil by sour ore deposit mass ratio, stirs, and adds ANTIMONY TRIOXIDE SB 203 99.8 PCT (Sb according to the ratio of 1-20kg/ ton new technological process titanium slag
2O
3), mix, adding entry conditioned reaction acid concentration is 93-96%, stop heating after under agitation being warming up to 130-150 ℃, make spontaneous the carrying out of reaction, generate solid mixt, solid mixt is placed 160-220 ℃ of following slaking 3-5h, by water ore deposit mass ratio is 2.5-3: 1 adds the water extraction solid mixt, and leaching temperature is 60-75 ℃, and leaching time is 1-3h;
(2), sedimentation removal of impurities:
Ratio in 10-40kg/ ton new technological process titanium slag in step (1) gained acid hydrolysis solution adds FeS, and the ANTIMONY TRIOXIDE SB 203 99.8 PCT that adds when FeS and acidolysis forms sinking agent, and sedimentation goes out most chromium metal, vanadium in the acid hydrolysis solution; Add flocculation agent again, make short grained solid impurity sedimentation, after solid-liquid separation, obtain titanium liquid clearly, in clear titanium liquid, add aluminum removal, freezing and crystallizing 1-2h under 10-20 ℃ temperature, add aluminum removal molar weight be Tai-Ace S 150 mole number in the solution 1.0-1.5 doubly;
The separation of freezing and crystallizing after-filtration obtains crystal and titanium concentration is the titanium liquid of 110-140g/L, adds oxygenant in described titanium liquid, makes the concentration of the titanous in the titanium liquid reduce to 1-2g/L by 5-20g/L; Gained liquid obtains the dense titanium liquid that concentration is 200-235g/L through concentrating after the oxidation;
(3), hydrolysis:
Adding automatic growing crystal species or plus seed are hydrolyzed in the dense titanium liquid of step (2) gained, and wherein the quality of crystal seed that plus seed adds is TiO in the titanium liquid
2The 1-3% of quality; Titanium liquid initial reaction concentration is 180-195g/L, and the temperature that adds crystal seed is 90-95 ℃;
(4), filter, wash:
With the hydrolysis slurry filtration of step (3) gained, the filter cake that obtains obtains the rutile titanium white powder after bleaching, salt processing, calcining, aftertreatment.
2. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that:
Sour ore deposit mass ratio in the step (1) is 1.67-1.75, and reaction acid concentration is 95%-96%, and the curing time is 3-4h.
3. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that:
Flocculation agent described in the step (2) is the poly-propionic acid amide of formaldehyde dimethylammonium modification, and its consumption is 15-30ppm.
4. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that:
Aluminum removal is ammonium sulfate or vitriolate of tartar described in the step (2), and it is Tai-Ace S 150 or potassium aluminium sulfate crystal that the freezing and crystallizing after-filtration separates the crystal that obtains.
5. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that: oxygenant is Sodium Nitrite or SODIUMNITRATE described in the step (2).
6. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that:
The quality of crystal seed that plus seed adds is TiO in the titanium liquid in the step (3)
2The 1.5-2.5% of quality.
7. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 6 is characterized in that: adding crystal seed in the step (3) is the plus seed titanium tetrachloride.
8. the method for utilizing the new technological process titanium slag to prepare the rutile titanium white powder according to claim 1 is characterized in that: new technological process titanium slag preferred powder described in the step (1) is broken to greater than 45 microns proportion of particles less than 15%.
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Address after: 618209 new industrial concentrated development zone, Sichuan, Mianzhu Patentee after: Longbai Sichuan Titanium Co., Ltd Address before: 618209 new industrial concentrated development zone, Sichuan, Mianzhu Patentee before: SICHUAN LOMON TITANIUM Co.,Ltd. |